CN109092314B - LaFe1-xCuxO3Perovskite material and preparation method - Google Patents
LaFe1-xCuxO3Perovskite material and preparation method Download PDFInfo
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Abstract
LaFe1‑xCuxO3A perovskite material obtained by the following process: step 1: separately weighing La (NO)3)3·6H2O、Fe(NO3)3·9H2O、Cu(NO3)2·3H2O and C6H8O7·H2O, dissolving in water, and stirring under the water bath heating condition to obtain wet gel; wherein La (NO)3)3·6H2O、Fe(NO3)3·9H2O、Cu(NO3)2·3H2O and C6H8O7·H2The molar ratio of O is 1 (1-x) x is 6, wherein x is 0.1, 0.2, 0.3, 0.4 or 0.5; step 2: drying the wet gel in a vacuum drying oven; and step 3: calcining at the temperature of 650-700 ℃ after presintering at the temperature of 350-450 ℃ to obtain the target product. The invention also discloses a preparation method of the material.
Description
Technical Field
The invention belongs to the technical field of water pollution control, and particularly relates to LaFe1-xCuxO3A perovskite material.
The invention also relates to a preparation method of the material.
Background
The general formula of the perovskite type oxide is ABO3The A site is generally rare earth or alkaline earth element ion, and the B site is transition element ion. The rare earth reserves and the output of China are the first in the world, but the rare earth utilization rate is low. The rare earth element has the characteristics of an unfilled 4f electronic layer, lanthanide contraction and the like, has excellent oxygen storage and release capacity and mechanical stability, and researches show that the introduction of the rare earth has an obvious promotion effect on the catalytic performance of the transition metal oxide. The catalyst also has high thermal stability and chemical corrosion resistance, and has been reported by Nature et al as a catalytic material with great industrial application prospect. In view of this, rare earth element La is introduced to prepare perovskite type metal oxide, and the B site of the perovskite type metal oxide is partially doped, so that the catalytic activity of the transition metal oxide in the heterogeneous catalysis of persulfate oxidation water for degradation-resistant organic pollutants can be remarkably improved, and the technology has wide application prospect.
Disclosure of Invention
The invention aims to provide a LaFe1-xCuxO3A perovskite material.
It is a further object of the present invention to provide a method for preparing the above material.
In order to achieve the purpose, the invention provides LaFe1-xCuxO3The perovskite material is an agglomerated nanoscale granular solid and is obtained by the following method:
step 1: separately weighing La (NO)3)3·6H2O、Fe(NO3)3·9H2O、Cu(NO3)2·3H2O and C6H8O7·H2O, dissolving in water, and stirring under the water bath heating condition to obtain wet gel; wherein La (NO)3)3·6H2O、Fe(NO3)3·9H2O、Cu(NO3)2·3H2O and C6H8O7·H2The molar ratio of O is 1 (1-x) x is 6, wherein x is 0.1, 0.2, 0.3, 0.4 or 0.5;
step 2: drying the wet gel in a vacuum drying oven;
and step 3: calcining at the temperature of 650-700 ℃ after presintering at the temperature of 350-450 ℃ to obtain the target product.
The LaFe1-xCuxO3In the perovskite material, the water is added in an amount such that the total concentration of metal ions is not higher than 0.02 mol/L.
The LaFe1-xCuxO3In the perovskite material, the specific surface area is 13.8-18.8m2Per g, the average particle diameter is 15-38nm, and the average pore diameter is 14.3-18.2 nm.
The invention provides the preparation of the LaFe1-xCuxO3The preparation method of the perovskite material comprises the following steps:
step 1: separately weighing La (NO)3)3·6H2O、Fe(NO3)3·9H2O、Cu(NO3)2·3H2O and C6H8O7·H2O, dissolving in water, and stirring under the water bath heating condition to obtain wet gel; wherein La (NO)3)3·6H2O、Fe(NO3)3·9H2O、Cu(NO3)2·3H2O and C6H8O7·H2The molar ratio of O is 1 (1-x) x is 6, wherein x is 0.1, 0.2, 0.3, 0.4 or 0.5;
step 2: drying the wet gel in a vacuum drying oven;
and step 3: calcining at the temperature of 650-700 ℃ after presintering at the temperature of 350-450 ℃ to obtain the target product.
In the preparation method, the water is added in an amount that the total concentration of metal ions is not higher than 0.02 mol/L.
In the preparation method, the temperature of the water bath in the step 1 is 85-95 ℃.
In the preparation method, the drying temperature of the step 2 is 95-120 ℃.
In the preparation method, the pre-sintering time in the step 3 is 4-5h, the calcining time is 4-5h, and the heating rate is 4-7 ℃/min.
The LaFe provided by the invention1-xCuxO3The perovskite material mayThe method is used for activating persulfate to treat residual atrazine in a water body.
Compared with the prior art, the invention has the following beneficial effects: the perovskite catalyst LaFe of the invention1-xCuxO3Has smaller grain diameter, larger aperture and specific surface area, uniform grain diameter appearance, and Fe and Cu can be used as active sites of catalytic reaction and LaFeO3Compared with the method which can activate persulfate more efficiently and generate SO with high oxidation activity4The method can be used for removing the pesticide pollutants difficult to degrade, remarkably improving the water quality, ensuring the water quality safety, and having high stability and no secondary pollution. With cheap and easily available La (NO)3)3·6H2O、Fe(NO3)3·9H2O、Cu(NO3)2·3H2O is used as a main preparation raw material, and LaFe which can be used as a catalyst for activating persulfate to treat residual atrazine in water body is prepared through the procedures of water bath, gelling, drying, calcining and grinding1-xCuxO3A perovskite material.
Drawings
FIG. 1 shows the prepared LaFe0.8Cu0.2O3A Scanning Electron Microscope (SEM) spectrum of the perovskite material.
FIG. 2 shows the prepared LaFe0.8Cu0.2O3A high resolution transmission electron microscope (HR-TEM) profile of the perovskite material.
Figure 3 shows the degradation of atrazine with different catalyst materials.
Detailed Description
The invention discloses a perovskite material capable of being used for activating persulfate to treat residual atrazine in a water body and a preparation method thereof. The invention specifically comprises the following steps:
step 1, respectively weighing a certain amount of La (NO)3)3·6H2O、Fe(NO3)3·9H2O、 Cu(NO3)2·3H2O and C6H8O7·H2O, dissolving in water, stirring at 85-95 deg.C under heating in water bathStirring for 2h to obtain wet gel;
step 2, placing the mixture in a vacuum drying oven for 6-8 hours and drying the mixture;
step 3, placing the material in a muffle furnace, pre-burning for 4-5h at medium temperature, and then calcining for 4-5h at high temperature to obtain a target product LaFe1-xCuxO3Perovskite material, the material obtained by calcining is ground into uniform fine particles for standby.
The perovskite material of the invention has a specific surface area of 13.8-18.8m2Per g, the average particle diameter is 15-38nm, and the average pore diameter is 14.3-18.2 nm.
Preferably, in step 1, La (NO)3)3·6H2O、Fe(NO3)3·9H2O、Cu(NO3)2·3H2O and C6H8O7·H2The molar ratio of O is 1 (1-x) x:6, wherein x is 0.1, 0.2, 0.3, 0.4 or 0.5.
Preferably, in step 1, the amount of water added is such that the total concentration of metal ions is not higher than 0.02 mol/L.
Preferably, in step 2, the drying temperature is 95 ℃.
Preferably, in step 3, the pre-firing temperature is 400 ℃ and the post-firing temperature is 700 ℃.
Preferably, in the step 3, the temperature rise rate of the muffle furnace is 4-7 ℃/min.
The present invention will be described in detail with reference to examples and comparative examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
Step one, respectively weighing La (NO) according to the molar concentration ratio of 1:0.9:0.1:63)3·6H2O、 Fe(NO3)3·9H2O、Cu(NO3)2·3H2O and C6H8O7.H2O，Adding water to dissolve the metal ions so that the total concentration of the metal ions is 0.02mol/L, and stirring for 2 hours under the water bath heating condition of 85 ℃ to obtain wet gel;
step two, placing the mixture in a vacuum drying oven for 6 hours to dry the mixture, wherein the drying temperature is 95 ℃;
thirdly, placing the material in a muffle furnace, pre-sintering for 4 hours at 400 ℃, and then calcining for 4 hours at 700 ℃ to obtain catalyst powder, wherein the heating rate of the muffle furnace is 4 ℃/min;
and step four, grinding the calcined material to uniform fine particles for later use.
Example 2
Step one, respectively weighing La (NO) according to the molar concentration ratio of 1:0.8:0.2:63)3·6H2O、Fe(NO3)3·9H2O、Cu(NO3)2·3H2O and C6H8O7.H2O, adding water to dissolve the metal ions so that the total concentration of the metal ions is 0.02mol/L, and stirring for 2 hours under the water bath heating condition of 90 ℃ to obtain wet gel;
step two, placing the mixture in a vacuum drying oven for 7 hours for drying, wherein the drying temperature is 95 ℃;
thirdly, placing the material in a muffle furnace, pre-sintering for 4h at 400 ℃, and then calcining for 5h at 700 ℃ to obtain catalyst powder, wherein the heating rate of the muffle furnace is 5 ℃/min;
and step four, grinding the calcined material to uniform fine particles for later use.
Example 3
Step one, respectively weighing La (NO) according to the molar concentration ratio of 1:0.7:0.3:63)3·6H2O、 Fe(NO3)3·9H2O、Cu(NO3)2·3H2O and C6H8O7.H2O, adding water to dissolve the metal ions so that the total concentration of the metal ions is 0.02mol/L, and stirring for 2 hours under the water bath heating condition of 95 ℃ to obtain wet gel;
step two, placing the mixture in a vacuum drying oven for 8 hours to dry the mixture, wherein the drying temperature is 95 ℃;
thirdly, placing the material in a muffle furnace, pre-sintering the material for 5 hours at 400 ℃, and then calcining the material for 5 hours at 700 ℃ to obtain catalyst powder, wherein the heating rate of the muffle furnace is 6 ℃/min;
and step four, grinding the calcined material to uniform fine particles for later use.
Example 4
Step one, respectively weighing La (NO) according to the molar concentration ratio of 1:0.6:0.4:63)3·6H2O、 Fe(NO3)3·9H2O、Cu(NO3)2·3H2O and C6H8O7.H2O, adding water to dissolve the metal ions so that the total concentration of the metal ions is 0.02mol/L, and stirring for 2 hours under the water bath heating condition of 85 ℃ to obtain wet gel;
step two, placing the mixture in a vacuum drying oven for 7 hours for drying, wherein the drying temperature is 95 ℃;
thirdly, placing the material in a muffle furnace, pre-sintering the material for 5 hours at 400 ℃, and then calcining the material for 4 hours at 700 ℃ to obtain catalyst powder, wherein the heating rate of the muffle furnace is 7 ℃/min;
and step four, grinding the calcined material to uniform fine particles for later use.
Example 5
Step one, respectively weighing La (NO) according to the molar concentration ratio of 1:0.5:0.5:63)3·6H2O、 Fe(NO3)3·9H2O、Cu(NO3)2·3H2O and C6H8O7.H2O, adding water to dissolve the metal ions so that the total concentration of the metal ions is 0.02mol/L, and stirring for 2 hours under the water bath heating condition of 90 ℃ to obtain wet gel;
step two, placing the mixture in a vacuum drying oven for 8 hours to dry the mixture, wherein the drying temperature is 95 ℃;
thirdly, placing the material in a muffle furnace, pre-sintering for 4 hours at 400 ℃, and then calcining for 4 hours at 700 ℃ to obtain catalyst powder, wherein the heating rate of the muffle furnace is 5 ℃/min;
and step four, grinding the calcined material to uniform fine particles for later use.
Comparative example 1
This comparative example andexample 1 differs in that: without addition of Cu (NO)3)2·3H2O, namely respectively weighing La (NO) according to the molar concentration ratio of 1:1:63)3·6H2O、Fe(NO3)3·9H2O, and C6H8O7·H2And O, adding water to dissolve the metal ions so that the total concentration of the metal ions is 0.02mol/L, and stirring for 2 hours under the water bath heating condition of 85 ℃ to obtain wet gel, and then carrying out subsequent operations.
Detecting the effect
The materials obtained in examples 1-5 and comparative example 1 were used as catalysts to carry out the water body residual atrazine persulfate activation degradation test.
The test method comprises the following steps: the ambient temperature is 25.0 +/-1.0 ℃, and the concentration of the atrazine in the water is 5 mg/L. The catalytic material was added in an amount of 0.5 g/l, and then a potassium hydrogen peroxymonosulfate solution was added to a concentration of 0.5 mmol/l. Stirring for 90 minutes, sampling and filtering at regular intervals, and detecting the concentration of the atrazine at a certain moment by high performance liquid chromatography.
LaFe prepared in example 2 was observed by scanning electron microscope0.8Cu0.2O3Perovskite material, it is found from figure 1 that the material is an agglomerated nanoscale particulate solid of uniform particle size.
LaFe prepared in example 2 was observed by high-resolution transmission electron microscope0.8Cu0.2O3The perovskite material can be seen from the electron micrograph of FIG. 2 as lattice stripes with a spacing of 0.284 nm.
FIG. 3 shows LaFe prepared by the present invention1-xCuxO3The effect diagram of removing pesticide atrazine in water by catalyzing potassium monopersulfate with the perovskite material is shown, wherein the atrazine in water can be completely degraded within 90 minutes in examples 2-5 except that the atrazine degradation rate within 90 minutes in example 1 is 70%. Comparative example LaFeO of lanthanum iron perovskite not doped with copper3The degradation efficiency in 90 minutes is 50%. The high-efficiency degradation capability of the material prepared by the method of the invention on the atrazine in water is shown.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (7)
1. LaFe1-xCuxO3The perovskite material is an agglomerated nano-grade granular solid with the specific surface area of 13.8-18.8m2(ii)/g, average particle diameter of 15-38nm, average pore diameter of 14.3-18.2nm, obtained by the following method:
step 1: separately weighing La (NO)3)3·6H2O、Fe(NO3)3·9H2O、Cu(NO3)2·3H2O and C6H8O7·H2O, dissolving in water, and stirring under the water bath heating condition to obtain wet gel; wherein La (NO)3)3·6H2O、Fe(NO3)3·9H2O、Cu(NO3)2·3H2O and C6H8O7·H2The molar ratio of O is 1 (1-x) x is 6, wherein x is 0.1, 0.2, 0.3, 0.4 or 0.5;
step 2: drying the wet gel in a vacuum drying oven;
and step 3: calcining at the temperature of 650-700 ℃ after presintering at the temperature of 350-450 ℃ to obtain the target product.
2. LaFe according to claim 11-xCuxO3A perovskite material, wherein the amount of added water is such that the total concentration of metal ions is not higher than 0.02 mol/L.
3. LaFe as defined in claim 11-xCuxO3The preparation method of the perovskite material comprises the following steps:
step 1: separately weighing La (NO)3)3·6H2O、Fe(NO3)3·9H2O、Cu(NO3)2·3H2O and C6H8O7·H2O, dissolving in water, and stirring under the water bath heating condition to obtain wet gel; wherein La (NO)3)3·6H2O、Fe(NO3)3·9H2O、Cu(NO3)2·3H2O and C6H8O7·H2The molar ratio of O is 1 (1-x) x is 6, wherein x is 0.1, 0.2, 0.3, 0.4 or 0.5;
step 2: drying the wet gel in a vacuum drying oven;
and step 3: calcining at the temperature of 650-700 ℃ after presintering at the temperature of 350-450 ℃ to obtain the target product.
4. The production method according to claim 3, wherein the amount of water added is such that the total concentration of metal ions is not more than 0.02 mol/L.
5. The method of claim 3, wherein the temperature of the water bath in step 1 is 85-95 ℃.
6. The preparation method according to claim 3, wherein the drying temperature in the step 2 is 95-120 ℃.
7. The preparation method according to claim 3, wherein the pre-sintering time of the step 3 is 4-5h, the calcining time is 4-5h, and the temperature rising rate is 4-7 ℃/min.
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